WO2018134348A1 - Optoelectronic device for detection of a substance dispersed in a fluid. - Google Patents

Optoelectronic device for detection of a substance dispersed in a fluid. Download PDF

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Publication number
WO2018134348A1
WO2018134348A1 PCT/EP2018/051296 EP2018051296W WO2018134348A1 WO 2018134348 A1 WO2018134348 A1 WO 2018134348A1 EP 2018051296 W EP2018051296 W EP 2018051296W WO 2018134348 A1 WO2018134348 A1 WO 2018134348A1
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WO
WIPO (PCT)
Prior art keywords
optoelectronic device
light radiation
optical
signals
light source
Prior art date
Application number
PCT/EP2018/051296
Other languages
French (fr)
Inventor
Carlo Guardiani
Original Assignee
E-Lite S.R.L.
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Filing date
Publication date
Application filed by E-Lite S.R.L. filed Critical E-Lite S.R.L.
Priority to US16/479,622 priority Critical patent/US11536720B2/en
Priority to EP18702939.2A priority patent/EP3571492B1/en
Priority to ES18702939T priority patent/ES2864600T3/en
Publication of WO2018134348A1 publication Critical patent/WO2018134348A1/en

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/53Immunoassay; Biospecific binding assay; Materials therefor
    • G01N33/543Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals
    • G01N33/54366Apparatus specially adapted for solid-phase testing
    • G01N33/54373Apparatus specially adapted for solid-phase testing involving physiochemical end-point determination, e.g. wave-guides, FETS, gratings
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/7703Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator using reagent-clad optical fibres or optical waveguides
    • G01N21/7746Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator using reagent-clad optical fibres or optical waveguides the waveguide coupled to a cavity resonator
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N2021/7769Measurement method of reaction-produced change in sensor
    • G01N2021/7776Index
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N2021/7769Measurement method of reaction-produced change in sensor
    • G01N2021/7789Cavity or resonator
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/10Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
    • G02B6/12Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
    • G02B2006/12133Functions
    • G02B2006/12138Sensor
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/10Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
    • G02B6/12Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
    • G02B6/12007Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind forming wavelength selective elements, e.g. multiplexer, demultiplexer

Definitions

  • the present invention relates to an optoelectronic device for detection of a substance dispersed in a fluid.
  • Some optoelectronic devices of known type use an open loop detection system to detect the target substance.
  • An optoelectronic device of this type is described in the patent application US2012/0092650.
  • the device described therein is provided with an optical circuit comprising one or more optical resonators, each of which comprises a ring optical path having an active surface capable of selectively absorbing the target substance.
  • the light emitted by a light source laser is transmitted, through the free space, to the optical circuit, conveyed through the optical resonators and transmitted, again through the free space, to a spectrum analyser.
  • the optical path of the light in optical resonators varies as a function of the quantity of target substance absorbed selectively by the active surface of these latter, the presence or concentration of the target substance can be detected by analysing the spectrum of the light transmitted by the optical circuit.
  • the measurement signal indicative of the presence or concentration of the target substance is typically characterized by a relatively high signal-to-noise ratio. Therefore, to obtain acceptable performance, very accurate control of the physical and optical characteristics of the components and of the environmental operating conditions (temperature, humidity and the like) is necessary. Consequently, practical use of these devices is often difficult and laborious.
  • This device is provided with an integrated photonic circuit comprising a pair or optical resonators arranged in series along an optical path.
  • the light emitted by a broad spectrum laser light source (for example of Fabry-Perot type) is transmitted, through the free space, to the integrated photonic circuit and conveyed to a first optical resonator arranged to operate as an optical filter (optionally with adjustable bandpass) having a transmittance peak at a specific wavelength.
  • a broad spectrum laser light source for example of Fabry-Perot type
  • a first optical resonator arranged to operate as an optical filter (optionally with adjustable bandpass) having a transmittance peak at a specific wavelength.
  • the light exiting from the first optical resonator is in part conveyed to a first photo-diode operatively connected to a control unit and in part transmitted to the second optical resonator.
  • This latter is provided with an optical path having an active surface capable of selectively absorbing the substance to be detected.
  • the light radiation traveling through the second resonator is subjected to a variation (shift) of the resonance wavelength, which is a function of the quantity of substance to be detected absorbed by the active surface of the resonator.
  • the light exiting from the second resonator is transmitted to a further photo-diode operatively connected to a control unit.
  • the control unit generates control signals (for example an electric current or voltage applied to the integrated photonic circuit) to align the wavelength of the transmittance peak of the first optical resonator with the resonance wavelength of the second optical resonator. These control signals are indicative of the presence or concentration of the substance to detect.
  • control signals for example an electric current or voltage applied to the integrated photonic circuit
  • Optoelectronic devices of the type described above without doubt offer improved performance in terms of accuracy and measurement resolution, with respect to more conventional devices.
  • the device described in the patent US9080953 requires the aforesaid resonators to have almost identical physical and optical characteristics to obtain satisfactory immunity from common mode noise. Moreover, it is necessary to provide a regulator to vary, in a controlled way, the resonance wavelength of at least one resonator by means of suitable current or voltage control signals. Therefore, it is difficult and costly to produce industrially.
  • the present invention intends to meet this need by providing an optoelectronic device according to claim 1 and the related dependent claims, set forth below.
  • FIG. 1-5 illustrate, by way of example, the structure and the operation of the optoelectronic device according to the invention.
  • the present invention relates to an optoelectronic device 1 for detection of the presence or concentration of a target substance dispersed in a fluid 50.
  • the target substance to be detected by means of the electronic device 1 , can be of any type, for example a material, a compound, a chemical or biological substance.
  • the fluid 50 can also be of any type: a liquid (for example of biological origin, a process liquid or a chemical solution) or a gas (for example a process gas).
  • a liquid for example of biological origin, a process liquid or a chemical solution
  • a gas for example a process gas
  • the optoelectronic device 1 comprises a light source 2 adapted to emit a light radiation L E having an adjustable wavelength Xs, for example with values in the order of nanometers.
  • the light source 2 is a laser light source, more particularly a laser source with very narrow spectrum (a few nm), for example a DFB laser.
  • the optoelectronic device 1 comprises an integrated electronic circuit 100 operative ly coupled to the light source 2.
  • the integrated electronic circuit 100 can advantageously be produced industrially with known techniques for processing semiconductor materials. For example, techniques for planar processing of integrated circuits, techniques for micro-machining silicon (bulk micro- machining or surface micro-machining), or the like can be used.
  • the integrated electronic circuit 100 can have dimensions in the order of tens or hundreds of ⁇ .
  • the integrated circuit 100 is structurally separate from the light source 2 and coupled operatively to this latter.
  • the light source 2 and the integrated circuit 100 could be structurally integrated with each other, optionally also in a single integrated circuit.
  • the optoelectronic device 1 comprises a control unit 9 operatively coupled to the light source 2 and to the integrated circuit 100.
  • the control unit 9 is an electronic device that comprises a plurality of functional modules 91 ,
  • these functional modules can comprise electronic circuits
  • these functional modules can comprise sets of software instructions, stored or storable on a data storage medium, and executable by one or more digital signal processing units (for example microprocessors) to perform the desired functions.
  • digital signal processing units for example microprocessors
  • the control unit 9 is easy to produce industrially with known electronic circuit assembly techniques (for example assembly on PCB).
  • control unit 9 and the integrated circuit 100 could be structurally integrated with each other, optionally also in a single integrated circuit.
  • the control unit 9 is adapted to provide control signals (of electric type) to the light source 2 to adjust the wavelength s of the light radiation L E emitted by this latter.
  • control unit 9 is also adapted to carry out signal processing functions and to provide first measurement signals M indicative of a presence or concentration of the target substance dispersed in the fluid 50.
  • the integrated electronic circuit 100 comprises an integrated photonic circuit 10 operatively coupled to the light source 2.
  • the photonic circuit 10 comprises an optical coupler 3, preferably of the grating type (optical grating coupler).
  • the optical coupler 3 is operatively coupled to the light source 2 and is adapted to receive a light radiation L E emitted by the light source 2 and transmit a light radiation L T .
  • the optical coupler 3 is provided with a first active surface 31 optically coupled with the light source 2.
  • the optoelectronic device 1 comprises a first wave-guide 1 1 to optically couple the optical coupler 3 with the light source 2.
  • the optical coupler 3 is advantageously formed by a corresponding portion of the photonic circuit 10 suitably processed, for example by means of know techniques for processing semiconductor materials.
  • the active surface 31 can have an extension about 10 ⁇ 2 .
  • the wave-guide 1 1 comprises an optical fiber, for example of single mode type
  • the photonic circuit 10 comprises a first detector 4 and an optical resonator 5 optically coupled with the optical coupler 3 and a second detector 6 optically coupled with the optical resonator 5.
  • the first detector 4 is adapted to receive a first light radiation L- ⁇ transmitted by the optical coupler 3, which, in general, corresponds to a first portion of the light radiation L T transmitted by said optical coupler.
  • the optical resonator 5 is adapted to convey and transmit a second light radiation L T2 , which, in general, corresponds to a second portion of the light radiation L T transmitted by the optical coupler 3.
  • the second detector 6 is adapted to receive the second light radiation L T2 transmitted by the optical resonator 5.
  • first and second portions L T i, L T2 of the light radiation L T transmitted by the optical coupler 3 are complementary one to another (in quantitative terms).
  • the quantitative value of said first and second portions of light radiation L TI , L T2 basically depends on the wavelength of the light radiation L T transmitted by the optical coupler 3.
  • the first portion of light radiation L TI received by the detector 4 has a maximum value whereas the second portion of light radiation L T2 conveyed by the optical resonator 5 and transmitted to the second detector 6 has a minimum value.
  • the first portion of light radiation L TI may substantially correspond to the full amount light radiation L T transmitted by the optical coupler 3 whereas the second portion of light radiation L T2 may be substantially null.
  • the first portion of light radiation L TI received by the detector 4 has a minimum value (which may be substantially null) whereas the second portion of light radiation L T2 conveyed by the optical resonator 5 and transmitted to the second detector 6 has a maximum value (which may substantially correspond to the full amount of light radiation L T transmitted by the optical coupler 3).
  • the second portion of light radiation L T2 may substantially correspond to the full amount light radiation L T transmitted by the optical coupler 3 whereas the first portion of light radiation L TI may be substantially null.
  • the optoelectronic device 1 comprises a second wave-guide 12 to optically couple the optical coupler 3 with the detector 4 and the optical resonator 5.
  • the wave-guide 12 is formed by a corresponding portion of the photonic circuit 10 suitably processed, for example by means of known techniques for processing semiconductor materials.
  • the wave-guide 12 can have a width of around 0.5 ⁇ and a length of a few tens of ⁇ .
  • the detector 4 is adapted to receive the first light radiation L T i and provide first detection signals S 1 (of electric type) indicative of the optical power SA of the said light radiation.
  • the detector 4 is operatively coupled with the control unit 9 to transmit the aforesaid detection signals SI to this latter.
  • the detector 4 comprises a photo-diode, advantageously formed by a corresponding portion of the photonic circuit 10 suitably processed, for example by means of known techniques for processing semiconductor materials.
  • the operative coupling between the detector 4 and the control unit 9 can also be produced using known techniques for electrically coupling integrated circuits and electronic devices.
  • the optical resonator 5 comprises a ring optical path 51 (ring optical resonator).
  • the optical resonator 5 is adapted to convey the light radiation L T2 along the ring optical path 51 and transmit said light radiation to the detector 6.
  • the optical resonator 5 is provided with a second active surface 52 destined to come into contact with the fluid 50.
  • the active surface 52 of the optical resonator 5 comprises a material capable of selectively absorbing the target substance to be detected.
  • This material can be of known type.
  • the resonance wavelength ⁇ of the optical resonator 5 varies as a function of the quantity of target substance absorbed by the active surface 52.
  • the resonance wavelength ⁇ of the optical resonator 5 can be expressed by the relation:
  • neff is the refraction index of the material at the active surface 52 and m is an integer (1 , 2, 3, 4).
  • Absorption of the target substance by the active surface 52 of the optical resonator 5 thus determines a variation (shift) A S HIFT of the resonance wavelength ⁇ of the light radiation L T2 that travels along the optical path 51.
  • Aneff is the variation of the refraction index due to the material absorbed at the active surface 52.
  • the optical resonator 5 is formed by a corresponding portion of the photonic circuit 10 suitable processed, for example by means of known techniques for processing semiconductor materials.
  • the optical resonator 5 can have a ring optical path 51 with radius r around 50 ⁇ .
  • the second detector 6 is adapted to receive the second light radiation L T2 and provide second detection signals S2 (of electrical type) indicative of the optical power S B of said light radiation L T2 .
  • the optoelectronic device 1 comprises a third wave-guide 13 to optically couple the optical resonator 5 with the second detector 6.
  • the wave-guide 13 is formed by a corresponding portion of the photonic circuit 10 suitably processed, for example by means of known techniques for processing semiconductor materials.
  • the wave-guide 13 can have a width of around 0.5 ⁇ and a length of a few tens of ⁇ .
  • the second detector 6 is operatively coupled with the control unit 9 to transmit the aforesaid detection signals S2 to this latter.
  • the second detector 6 comprises a photo-diode, advantageously formed by a corresponding portion of the photonic circuit 10 suitably processed, for example by means of known techniques for processing semiconductor materials.
  • the operative coupling between the second detector 6 and the control unit 9 can also be produced using known techniques for electrically coupling integrated circuits and electronic devices.
  • the optoelectronic device 1 comprises a first control loop 901 to adjust the wavelength s of the light radiation LE emitted by the light source 2.
  • control loop 901 comprises the photonic circuit 10 and a measurement module 91 , a signal processing module 92 and a first control module 93 of the control unit 9.
  • the measurement module 91 is operatively associated with the detectors 4, 6.
  • the measurement module 91 is adapted to receive the first and second detection signals S I , S2 and to provide, in response to said first and second detection signals, second measurement signals AS M indicative of a difference of optical power AS between the light radiations L T1 , L T2 received respectively by the detectors 4, 6.
  • the measurement module 91 can be a summing module arranged to receive in inverted format one of the detection signals S 1 , S2 (for example the signal S2).
  • the signal processing module 92 is operatively associated with the measurement module 91 .
  • the signal processing module 92 is adapted to receive the measurement signals ASM and to provide, in response to said measurement signals, regulation signals R indicative of a reference wavelength for the light source 2.
  • the signal processing module 92 advantageously comprises a trans-impedance amplifier module 921 and an integrator module 922 arranged in cascade, as illustrated in Fig. 1 .
  • the first control module 93 is operatively associated with the signal processing module 92.
  • the control module 93 can comprise a controller for a light source laser.
  • control unit 9 is adapted to provide, in response to the aforesaid detection signals S I , S2, also first measurement signals M indicative of a presence or concentration of the target substance.
  • the measurement signals M can be provided directly by the signal processing module 92, as illustrated in Fig. 1 .
  • the measurement signals M can be provided by a further signal processing module (not illustrated) of the control unit 9, which can advantageously be arranged to receive the detection signals S I , S2 and to provide, in response to said detection signals, the second measurement signals M.
  • FIGS. 2 and 3 schematically illustrate operation of the control loop 901 of the control unit 9.
  • This figure schematically shows the trend of the optical power curves SA, SB for the light radiations L T i, L T2 received by the detectors 4, 6 (when the control loop 901 is active) and the optical power curve Ss of the light radiation emitted by the light source 2.
  • optical power curves S A , S b can advantageously be calculated according to the following relations that express a physical-mathematical model of known type (lorentzian profile) for the optical resonator 5 (Fig. 2):
  • PA, PB are respectively the maximum optical power of the light radiation L- ⁇ and the minimum optical power of the light radiation L T2 .
  • the optical power curves SA, SB are substantially complementary with respect to the optical power curve Ss.
  • the optical power curves SA, SB in fact show periodic resonance peaks, at multiple wavelengths of the resonance wavelength ⁇ of the optical resonator 5.
  • neff is the refraction index of the material at the active surface 52 and r is the resonance wavelength of the optical resonator 5.
  • is the resonance wavelength of the optical resonator 5
  • is the width of the related resonance peak
  • the control unit thus provides a fully differential control of the wavelength Xs of the light radiation emitted by light source 2. This is an important advantage of the invention as it allows achieving an improved common mode noise rejection with respect to known solutions of the state of the art.
  • the crossing point P-lock between the optical power curves SA, S b is around the point of maximum slope of the optical power curves SA, SB. This allows maximization of the feedback gain and a further optimization of the common mode noise rejection. Moreover, unlike known solutions, for example the solution proposed by the patent US9080953, the response time takes minimum values at the wavelength ⁇ -lock.
  • absorption of the target substance by the active surface 52 of the optical resonator 5 determines a variation (shift) A SHIFT of the resonance wavelength ⁇ of the optical resonator and, consequently, a corresponding variation of the wavelength of the light radiation LT 2 that travels along the optical path 51.
  • a SHIFT depends on the quantity of target substance absorbed by the material of the active surface 52, as illustrated above.
  • the first wave-guide 1 1 comprises a movable end 1 1 1 in proximal position with respect to the first active surface 31 of the optical coupler 3.
  • the optoelectronic device 1 comprises an actuation device 8 operatively coupled to the movable end 111 of the wave-guide 11 to move this movable end along the motion plane ⁇ .
  • the actuation device 8 can be a micro-motor of stepping type capable of moving the movable end 111 of the wave-guide 11 with movements in the order of the 100 nm.
  • the optoelectronic device 1 comprises a second control loop 902 comprising the photonic circuit 10 and a second control module 94 of the control unit 9 operatively connected to the detector 4 to receive the detection signals SI provided by these latter.
  • the control module 94 is adapted to receive the detection signals SI and to provide, in response to the aforesaid detection signals, second control signals C2 for the actuation device 8 to move the movable end 111 of the wave-guide 11 and adjust the position of this latter at least along the motion plane ⁇ .
  • the inventors have verified how the distance Z0 of the motion plane ⁇ from the active surface 31 is not critical in order to optimize the transfer of optical power from the light source 2 to the optical coupler 3.
  • the movement of the movable end 111 can thus take place on a plane rather than three dimensions, with considerable advantages in terms of simple construction and positioning precision.
  • control unit 9 is adapted to execute a calibration procedure of the position of the movable end 111 of the wave-guide 11 (Fig. 5).
  • the calibration procedure is executed by the second control loop 902.
  • the calibration procedure is executed with the first control loop 901 deactivated and with the light source 2 that initially emits a light radiation L E having a calibration wavelength start at which the optical power SI of the first light radiation L-n received by the first detector 4 takes a maximum absolute value (Fig. 2).
  • the wavelength start can be obtained acting directly on the light source 2 (for example by means of the control module 93) or on a thermoregulation circuit operatively coupled to the photonic circuit 10.
  • the movement of the movable end 111 is implemented with stepping movements (positive or negative in the order of 100 nm) repeated cyclically until reaching the optimal calibration position along the respective motion axis.
  • the optoelectronic device 1 is provided with a control arrangement to control the temperature of the integrated circuit 100.
  • the optoelectronic device 1 comprises a temperature sensor circuit 71 (preferably integrated with the photonic circuit 10) adapted to provide third detection signals T (of electrical type) indicative of the temperature of the integrated circuit 100.
  • the optoelectronic device 1 comprises a control module 95 (preferably comprised in the control unit 9) and a heating circuit 70 operatively coupled to the integrated circuit 100 to heat this latter, when required.
  • the heating circuit 70 comprises one or more Peltier cells operatively coupled to a voltage source (for example the control unit 9) capable of providing a suitable regulation voltage for the aforesaid cells.
  • a voltage source for example the control unit 9
  • the control module 95, the temperature sensor circuit 71 and heater 70 form a third control loop 903 for regulating the temperature of the integrated circuit 100.
  • control module 95 is operatively connected to the temperature sensor 71 to receive the detection signals T provided by these latter.
  • the control module 94 is adapted to receive the detection signals T and to provide, in response to the aforesaid detection signals, third control signals C3 for the heating circuit 70.
  • the integrated electronic circuit 100 comprises a multilayer structure 100A made of semiconductor material, for example Si (Fig. 4).
  • the multilayer structure 100A can be produced by means of known techniques for processing semiconductor materials, for example SOI (Silicon On Insulator) wafers.
  • SOI Silicon On Insulator
  • the multilayer structure 100 A comprises a substrate 30 made of semiconductor material (for example Si-bulk having a thickness generally variable from 600um to 200um)
  • the multilayer structure 100A comprises a layer of insulating material 20 (for example Si0 2 ) superimposed on the substrate 30.
  • the layer of insulating material can be formed by a Buried Oxide Layer of a wafer of SOI type with a thickness comprised between 750 nm and 2 ⁇ .
  • the multilayer structure 100 A comprises a layer of semiconductor material 10A (for example Si-epi with a thickness between 300 nm and 2 ⁇ ) superimposed on the layer of insulating material 20.
  • semiconductor material 10A for example Si-epi with a thickness between 300 nm and 2 ⁇
  • the integrated photonic circuit 10 is advantageously produced at the layer 10A.
  • the layer 10A of the multilayer structure 100A thus advantageously comprises, in the form of integrated circuits, at least the optical coupler 3, the optical resonator 5, the waveguides 12, 13 and the detectors 4, 6.
  • the temperature sensor circuit 71 is also integrated with the photonic circuit 10 and is produced at the layer 10A of the multilayer structure 100A.
  • the integrated electronic circuit 100 comprises a protective layer 40 made of plastic material superimposed on the layer 10A of the multilayer structure 100A.
  • the protective layer 40 is advantageously provided with suitable openings to allow the fluid
  • the optoelectronic device according to the invention has considerable advantages with respect to state of the art devices.
  • the optoelectronic device 1 uses a single optical resonator 5 to generate an error signal of differential type used by the control loop 901 to control the light source 2. This allows a high rejection of any common mode noise (for example due to variations of temperature, vibrations, etc.) to be obtained, with consequent increase of the accuracy and of the measurement resolution.
  • the optoelectronic device 1 is advantageously provided with a motion system of the waveguide 11 that couples the light source 2 with the photonic circuit 10. It is thus possible to considerably reduce the coupling losses due to any misalignments between the light cone emitted by the wave-guide 11 and the active surface 31 of the optical coupler 3.
  • the optoelectronic device 1, in particular the photonic circuit 10, and more generally the integrated circuit 100, is particularly suitable for mass production (batch processing) by means of known techniques for processing semiconductor materials. Moreover, the integrated circuit 100, in particular the photonic circuit 10, is easy to operatively couple with the control unit 9. The optoelectronic device 1 therefore has a very compact structure, easy to produce industrially at relatively limited costs.
  • the optoelectronic device 1 is particularly suitable for use in an apparatus for the detection of substances dispersed in a fluid or in an apparatus of bio-medical type.
  • An apparatus of this type may comprise, for example, a sample preparation unit to collect a process fluid to analyse, a micro-fluidic chamber and a peristaltic pump to force the collected process fluid to flow from the sample preparation unit into the micro-fluidic chamber.
  • the process fluid is brought into contact with the active surface of the optoelectronic device 1.
  • the process fluid is conveniently pumped into the microfluidic chamber with suitable speed and flow in order to maximize the binding probability of possible low-concentration target molecules with the active surface 52 of the optoelectronic device 1.
  • the measurement signals M (which may be indicative of a concentration value or a binding event count) provided by the optoelectronic device 1 may be conveniently processed to obtain an analyte concentration metric by a suitable data-analysis software.
  • the optoelectronic device 1 ensures high performance in terms of accuracy and measurement resolution. For example, it is capable of detecting dispersed substances with very low concentration values, for example tens of particles (of dimensions below 100 nm) per millilitre (ml). For many types of target substances, the optoelectronic device 1 is able to offer a numerical count of the molecules in a fluid.

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Abstract

The present invention relates to an optoelectronic device (1) for detection of a target substance dispersed in a fluid (50). The optoelectronic device comprises: ‐ a light source (2) adapted to emit a light radiation (LE) having an adjustable wavelength λs; - an integrated electronic circuit (100) comprising a photonic circuit (10) operatively coupled to said light source; - a control unit (9) operatively coupled to said light source and to said photonic circuit.

Description

OPTOELECTRONIC DEVICE FOR DETECTION
OF A SUBSTANCE DISPERSED IN A FLUID DESCRIPTION
The present invention relates to an optoelectronic device for detection of a substance dispersed in a fluid.
In the state of the art, numerous examples of optoelectronic devices for detection of a target substance dispersed in a fluid are known.
Some optoelectronic devices of known type use an open loop detection system to detect the target substance.
An optoelectronic device of this type is described in the patent application US2012/0092650. The device described therein is provided with an optical circuit comprising one or more optical resonators, each of which comprises a ring optical path having an active surface capable of selectively absorbing the target substance.
The light emitted by a light source laser is transmitted, through the free space, to the optical circuit, conveyed through the optical resonators and transmitted, again through the free space, to a spectrum analyser.
Given that the optical path of the light in optical resonators varies as a function of the quantity of target substance absorbed selectively by the active surface of these latter, the presence or concentration of the target substance can be detected by analysing the spectrum of the light transmitted by the optical circuit.
Experience has shown how optoelectronic devices of the type indicated have numerous limitations in terms of accuracy and measurement resolution.
In fact, in these devices the measurement signal indicative of the presence or concentration of the target substance is typically characterized by a relatively high signal-to-noise ratio. Therefore, to obtain acceptable performance, very accurate control of the physical and optical characteristics of the components and of the environmental operating conditions (temperature, humidity and the like) is necessary. Consequently, practical use of these devices is often difficult and laborious.
Finally, the aforesaid currently available optoelectronic devices have numerous disadvantages in terms of structural complexity and overall dimensions and are relatively costly to achieve industrially, as they are somewhat unsuitable for production on an industrial scale in miniaturized format.
Other optoelectronic devices of known type use a closed loop detection system to detect the target substance. An optoelectronic device of this type is described in the patent US9080953.
This device is provided with an integrated photonic circuit comprising a pair or optical resonators arranged in series along an optical path.
The light emitted by a broad spectrum laser light source (for example of Fabry-Perot type) is transmitted, through the free space, to the integrated photonic circuit and conveyed to a first optical resonator arranged to operate as an optical filter (optionally with adjustable bandpass) having a transmittance peak at a specific wavelength.
The light exiting from the first optical resonator is in part conveyed to a first photo-diode operatively connected to a control unit and in part transmitted to the second optical resonator. This latter is provided with an optical path having an active surface capable of selectively absorbing the substance to be detected.
The light radiation traveling through the second resonator is subjected to a variation (shift) of the resonance wavelength, which is a function of the quantity of substance to be detected absorbed by the active surface of the resonator.
The light exiting from the second resonator is transmitted to a further photo-diode operatively connected to a control unit.
The control unit generates control signals (for example an electric current or voltage applied to the integrated photonic circuit) to align the wavelength of the transmittance peak of the first optical resonator with the resonance wavelength of the second optical resonator. These control signals are indicative of the presence or concentration of the substance to detect.
Optoelectronic devices of the type described above without doubt offer improved performance in terms of accuracy and measurement resolution, with respect to more conventional devices.
However, currently available devices of this type are typically difficult to use practically and complex to produce industrially.
For example, the device described in the patent US9080953 requires the aforesaid resonators to have almost identical physical and optical characteristics to obtain satisfactory immunity from common mode noise. Moreover, it is necessary to provide a regulator to vary, in a controlled way, the resonance wavelength of at least one resonator by means of suitable current or voltage control signals. Therefore, it is difficult and costly to produce industrially. The scientific papers "TriPleX-Based integrated Optical ring resonators for Lab-on-Chip and Environmental Detection", IEEE Journal of Selected Topics in Quantum Electronics, Vol. 18, n° 5, September 2012, pages 1583-1596 (XP011466307) by Heideman R. et al. and "Design and optimization of micro-ring resonators in biochemical sensing applications", Journal of Lightwave Technology, Vol. 24, n° 3, March 2006, pages 1395-1402 (XP055412235) by Chung- Yen Chao et al. and the patent document US9448181B2 disclose further known examples of optoelectronic devices including ring resonating sensors.
Unfortunately, also these devices do not allow to completely overcome the above-mentioned technical issues of the state of the art.
Nowadays, there is still great need to provide optoelectronic devices for detection of a target substance dispersed in a fluid capable of offering high performance in terms of accuracy, measurement resolution, response times and, at the same time, which are relatively simple to use practically and easy to produce industrially, in miniaturized format.
The present invention intends to meet this need by providing an optoelectronic device according to claim 1 and the related dependent claims, set forth below.
Further characteristics and advantages of the present invention will become more apparent with reference to the description given below and to the accompanying figures, provided purely for explanatory and non- limiting purposes, wherein Figs 1-5 illustrate, by way of example, the structure and the operation of the optoelectronic device according to the invention.
With reference to the aforesaid figures, the present invention relates to an optoelectronic device 1 for detection of the presence or concentration of a target substance dispersed in a fluid 50.
In principle, the target substance to be detected, by means of the electronic device 1 , can be of any type, for example a material, a compound, a chemical or biological substance.
The fluid 50 can also be of any type: a liquid (for example of biological origin, a process liquid or a chemical solution) or a gas (for example a process gas).
The optoelectronic device 1 comprises a light source 2 adapted to emit a light radiation LE having an adjustable wavelength Xs, for example with values in the order of nanometers. Preferably, the light source 2 is a laser light source, more particularly a laser source with very narrow spectrum (a few nm), for example a DFB laser.
The optoelectronic device 1 comprises an integrated electronic circuit 100 operative ly coupled to the light source 2.
The integrated electronic circuit 100 can advantageously be produced industrially with known techniques for processing semiconductor materials. For example, techniques for planar processing of integrated circuits, techniques for micro-machining silicon (bulk micro- machining or surface micro-machining), or the like can be used.
The integrated electronic circuit 100 can have dimensions in the order of tens or hundreds of μηι.
In the embodiments described below, the integrated circuit 100 is structurally separate from the light source 2 and coupled operatively to this latter.
However, in some embodiments of the optoelectronic device 1 , the light source 2 and the integrated circuit 100 could be structurally integrated with each other, optionally also in a single integrated circuit.
The optoelectronic device 1 comprises a control unit 9 operatively coupled to the light source 2 and to the integrated circuit 100.
The control unit 9 is an electronic device that comprises a plurality of functional modules 91 ,
92, 93, 94, 95 that can be produced industrially in analog and/or digital mode.
If produced in analog mode, these functional modules can comprise electronic circuits
(separated into distinct units or integrated with one another) arranged to perform the desired functions.
If produced digitally, these functional modules can comprise sets of software instructions, stored or storable on a data storage medium, and executable by one or more digital signal processing units (for example microprocessors) to perform the desired functions.
The control unit 9 is easy to produce industrially with known electronic circuit assembly techniques (for example assembly on PCB).
In some embodiments of the optoelectronic device 1 , the control unit 9 and the integrated circuit 100 could be structurally integrated with each other, optionally also in a single integrated circuit.
The control unit 9 is adapted to provide control signals (of electric type) to the light source 2 to adjust the wavelength s of the light radiation LE emitted by this latter.
Preferably, as will be more apparent below, the control unit 9 is also adapted to carry out signal processing functions and to provide first measurement signals M indicative of a presence or concentration of the target substance dispersed in the fluid 50.
According to the invention, the integrated electronic circuit 100 comprises an integrated photonic circuit 10 operatively coupled to the light source 2.
The photonic circuit 10 comprises an optical coupler 3, preferably of the grating type (optical grating coupler).
The optical coupler 3 is operatively coupled to the light source 2 and is adapted to receive a light radiation LE emitted by the light source 2 and transmit a light radiation LT.
To this end, the optical coupler 3 is provided with a first active surface 31 optically coupled with the light source 2. Preferably, the optoelectronic device 1 comprises a first wave-guide 1 1 to optically couple the optical coupler 3 with the light source 2.
The optical coupler 3 is advantageously formed by a corresponding portion of the photonic circuit 10 suitably processed, for example by means of know techniques for processing semiconductor materials.
For example, the active surface 31 can have an extension about 10 μιη2.
Preferably, the wave-guide 1 1 comprises an optical fiber, for example of single mode type
(SMF - Single Mode Fibers), having a core diameter of around 10 μιη.
The photonic circuit 10 comprises a first detector 4 and an optical resonator 5 optically coupled with the optical coupler 3 and a second detector 6 optically coupled with the optical resonator 5.
The first detector 4 is adapted to receive a first light radiation L-π transmitted by the optical coupler 3, which, in general, corresponds to a first portion of the light radiation LT transmitted by said optical coupler.
The optical resonator 5 is adapted to convey and transmit a second light radiation LT2, which, in general, corresponds to a second portion of the light radiation LT transmitted by the optical coupler 3. The second detector 6 is adapted to receive the second light radiation LT2 transmitted by the optical resonator 5.
In general, the above-mentioned first and second portions LTi, LT2 of the light radiation LT transmitted by the optical coupler 3 are complementary one to another (in quantitative terms). As it will better emerge from the following, the quantitative value of said first and second portions of light radiation LTI, LT2 basically depends on the wavelength of the light radiation LT transmitted by the optical coupler 3.
When the wavelength of the light radiation LT is far from the resonance wavelength λΓ of the optical resonator, the first portion of light radiation LTI received by the detector 4 has a maximum value whereas the second portion of light radiation LT2 conveyed by the optical resonator 5 and transmitted to the second detector 6 has a minimum value. In this case, the first portion of light radiation LTI may substantially correspond to the full amount light radiation LT transmitted by the optical coupler 3 whereas the second portion of light radiation LT2 may be substantially null.
When the wavelength of the light radiation LT is at the resonance wavelength λΓ of the optical resonator, the first portion of light radiation LTI received by the detector 4 has a minimum value (which may be substantially null) whereas the second portion of light radiation LT2 conveyed by the optical resonator 5 and transmitted to the second detector 6 has a maximum value (which may substantially correspond to the full amount of light radiation LT transmitted by the optical coupler 3). In this case, the second portion of light radiation LT2 may substantially correspond to the full amount light radiation LT transmitted by the optical coupler 3 whereas the first portion of light radiation LTI may be substantially null.
Preferably, the optoelectronic device 1 comprises a second wave-guide 12 to optically couple the optical coupler 3 with the detector 4 and the optical resonator 5.
Preferably, the wave-guide 12 is formed by a corresponding portion of the photonic circuit 10 suitably processed, for example by means of known techniques for processing semiconductor materials. For example, the wave-guide 12 can have a width of around 0.5 μιη and a length of a few tens of μιη.
The detector 4 is adapted to receive the first light radiation LTi and provide first detection signals S 1 (of electric type) indicative of the optical power SA of the said light radiation.
The detector 4 is operatively coupled with the control unit 9 to transmit the aforesaid detection signals SI to this latter.
Preferably, the detector 4 comprises a photo-diode, advantageously formed by a corresponding portion of the photonic circuit 10 suitably processed, for example by means of known techniques for processing semiconductor materials.
The operative coupling between the detector 4 and the control unit 9 can also be produced using known techniques for electrically coupling integrated circuits and electronic devices. The optical resonator 5 comprises a ring optical path 51 (ring optical resonator).
The optical resonator 5 is adapted to convey the light radiation LT2 along the ring optical path 51 and transmit said light radiation to the detector 6.
At least at one portion of the ring optical path 51 , the optical resonator 5 is provided with a second active surface 52 destined to come into contact with the fluid 50.
The active surface 52 of the optical resonator 5 comprises a material capable of selectively absorbing the target substance to be detected. This material can be of known type.
Given that the refraction index of the material at the optical path 51 varies when the active surface 52 absorbs a quantity of the target substance, the resonance wavelength λΓ of the optical resonator 5 varies as a function of the quantity of target substance absorbed by the active surface 52.
In fact, as is known, based on the known properties of ring optical resonators, the resonance wavelength λΓ of the optical resonator 5 can be expressed by the relation:
Figure imgf000008_0001
where r is the radius of the ring optical path 51 , neff is the refraction index of the material at the active surface 52 and m is an integer (1 , 2, 3, 4...)
Absorption of the target substance by the active surface 52 of the optical resonator 5 thus determines a variation (shift) A SHIFT of the resonance wavelength λΓ of the light radiation LT2 that travels along the optical path 51.
As is known, this variation A SHIFT can be expressed by the relation:
A uwT = λΓ * (Aneff/neff)
where Aneff is the variation of the refraction index due to the material absorbed at the active surface 52.
Preferably, the optical resonator 5 is formed by a corresponding portion of the photonic circuit 10 suitable processed, for example by means of known techniques for processing semiconductor materials. For example, the optical resonator 5 can have a ring optical path 51 with radius r around 50 μιη.
The second detector 6 is adapted to receive the second light radiation LT2 and provide second detection signals S2 (of electrical type) indicative of the optical power SB of said light radiation LT2.
Preferably, the optoelectronic device 1 comprises a third wave-guide 13 to optically couple the optical resonator 5 with the second detector 6.
Preferably, the wave-guide 13 is formed by a corresponding portion of the photonic circuit 10 suitably processed, for example by means of known techniques for processing semiconductor materials. For example, the wave-guide 13 can have a width of around 0.5 μιη and a length of a few tens of μιη.
The second detector 6 is operatively coupled with the control unit 9 to transmit the aforesaid detection signals S2 to this latter.
Preferably, the second detector 6 comprises a photo-diode, advantageously formed by a corresponding portion of the photonic circuit 10 suitably processed, for example by means of known techniques for processing semiconductor materials. The operative coupling between the second detector 6 and the control unit 9 can also be produced using known techniques for electrically coupling integrated circuits and electronic devices.
According to the invention, the control unit 9 is adapted to receive and process the first and second detection signals S I , S2 and to provide, in response to the aforesaid detection signals S I , S2, first control signals C I to adjust the wavelength s of the light radiation LE emitted by the light source 2 so that the difference of optical power AS = SA-SB between the light radiations LTi, LT2 takes a minimum value (for example AS = 0).
Preferably, the optoelectronic device 1 comprises a first control loop 901 to adjust the wavelength s of the light radiation LE emitted by the light source 2.
Preferably, the control loop 901 comprises the photonic circuit 10 and a measurement module 91 , a signal processing module 92 and a first control module 93 of the control unit 9.
The measurement module 91 is operatively associated with the detectors 4, 6.
The measurement module 91 is adapted to receive the first and second detection signals S I , S2 and to provide, in response to said first and second detection signals, second measurement signals ASM indicative of a difference of optical power AS between the light radiations LT1, LT2 received respectively by the detectors 4, 6. For example, the measurement module 91 can be a summing module arranged to receive in inverted format one of the detection signals S 1 , S2 (for example the signal S2).
The signal processing module 92 is operatively associated with the measurement module 91 . The signal processing module 92 is adapted to receive the measurement signals ASM and to provide, in response to said measurement signals, regulation signals R indicative of a reference wavelength for the light source 2.
Advantageously, the reference wavelength, calculated by the signal processing module 92, is a wavelength in the vicinity of a resonance wavelength λΓ of the optical resonator 5 at which the difference of optical power AS between the light radiations L-π, LT2 takes a minimum value (AS = 0).
Preferably, the signal processing module 92 advantageously comprises a trans-impedance amplifier module 921 and an integrator module 922 arranged in cascade, as illustrated in Fig. 1 .
The first control module 93 is operatively associated with the signal processing module 92. The first control module 93 is adapted to receive the regulation signals R and to provide, in response to said regulation signals, the first control signals C I to adjust the wavelength λ$ of the light radiation LE emitted by the light source 2 so that the difference of optical power AS between the light radiations L-π, LT2 takes a minimum value (AS = 0). For example, the control module 93 can comprise a controller for a light source laser.
Preferably, the control unit 9 is adapted to provide, in response to the aforesaid detection signals S I , S2, also first measurement signals M indicative of a presence or concentration of the target substance.
According to some embodiments of the invention, the measurement signals M can be provided directly by the signal processing module 92, as illustrated in Fig. 1 .
According to some embodiments of the invention, the measurement signals M can be provided by a further signal processing module (not illustrated) of the control unit 9, which can advantageously be arranged to receive the detection signals S I , S2 and to provide, in response to said detection signals, the second measurement signals M.
Figs. 2 and 3 schematically illustrate operation of the control loop 901 of the control unit 9.
This figure schematically shows the trend of the optical power curves SA, SB for the light radiations LTi, LT2 received by the detectors 4, 6 (when the control loop 901 is active) and the optical power curve Ss of the light radiation emitted by the light source 2.
The optical power curves SA, Sb can advantageously be calculated according to the following relations that express a physical-mathematical model of known type (lorentzian profile) for the optical resonator 5 (Fig. 2):
SA(X) = PA - (ΡΑΒ)/(1+(2(λ- λΓ)/ΔλΓ)2)
SBM = PB +(ΡΑΒ)/(1+(2(λ- λΓ)/ΔλΓ)2)
where PA, PB are respectively the maximum optical power of the light radiation L-π and the minimum optical power of the light radiation LT2.
As it is possible to observe from Fig. 2, the optical power curves SA, SB are substantially complementary with respect to the optical power curve Ss.
Given that the control loop 901 is active, the trend of both the optical power curves SA, SB is influenced by the action of the optical resonator 5.
The optical power curves SA, SB in fact show periodic resonance peaks, at multiple wavelengths of the resonance wavelength λΓ of the optical resonator 5.
Each resonance peak has a width ΔλΓ and a merit factor Q = (λΐ/Αλΐ).
The distance dr between two successive resonance peaks can be given by the relation:
dr = r2/(2nr*nejf)
where r is the radius of the ring optical path 51 , neff is the refraction index of the material at the active surface 52 and r is the resonance wavelength of the optical resonator 5.
As can be observed, according to the invention, in response to the first control signals CI provided by the control unit 9, the light source 2 emits a light radiation LE having a wavelength s such that the difference of optical power AS between the light radiations LTi, LT2 takes a minimum value (AS = 0).
It is evident how this condition is produced at a crossing point P-lock between the optical power curves SA, SB around the resonance wavelength λΓ of the optical resonator 5 (Fig. 2). The wavelength λ-lock corresponding to this crossing point is given by the following relation:
λ-lock = λΓ*(1- ΔλΓ/2λΓ) = r*(l-1/2Q)
where λΐ is the resonance wavelength of the optical resonator 5, ΔλΓ is the width of the related resonance peak and Q = r/A r) is the merit factor of the related resonance peak. The above clearly shows how the control unit 9 is adapted to control the light source 2 so that the wavelength Xs of the light radiation emitted by this latter continuously follows a wavelength (around the resonance wavelength Xr of the optical resonator 5) at which the difference of optical power AS between the light radiations L-π, LT2 takes a minimum value (AS = 0).
The control unit thus provides a fully differential control of the wavelength Xs of the light radiation emitted by light source 2. This is an important advantage of the invention as it allows achieving an improved common mode noise rejection with respect to known solutions of the state of the art.
It must be noted that the crossing point P-lock between the optical power curves SA, Sb is around the point of maximum slope of the optical power curves SA, SB. This allows maximization of the feedback gain and a further optimization of the common mode noise rejection. Moreover, unlike known solutions, for example the solution proposed by the patent US9080953, the response time takes minimum values at the wavelength λ-lock.
As indicated above, absorption of the target substance by the active surface 52 of the optical resonator 5 determines a variation (shift) A SHIFT of the resonance wavelength λΓ of the optical resonator and, consequently, a corresponding variation of the wavelength of the light radiation LT2 that travels along the optical path 51.
The extent of this variation A SHIFT depends on the quantity of target substance absorbed by the material of the active surface 52, as illustrated above.
In response to absorption of the target substance by the active surface 52 of the optical resonator 5, as illustrated in Fig. 3, the light source 2 thus emits a light radiation having a new wavelength -lock+A sHiFT, at which the difference of optical power AS between the light radiations LTi, LT2 takes a minimum value (AS = 0).
In practice, in response to an absorption of the target substance, there is a shift A SHIFT of the wavelength of the crossing point P-lock between the optical power curves SA, SB around the resonance wavelength λΓ of the optical resonator 5 (Fig. 3).
According to a preferred embodiment, illustrated in the aforesaid figures, the first wave-guide 1 1 comprises a movable end 1 1 1 in proximal position with respect to the first active surface 31 of the optical coupler 3.
Preferably, the movable end 1 1 1 of the wave-guide 1 1 is able to move at least along a motion plane π parallel to the first active surface 31 and at a predefined distance Z0 (for example Z0 = 15 μηι) from the active surface 31, according to an axis Z perpendicular to this latter.
Preferably, the optoelectronic device 1 comprises an actuation device 8 operatively coupled to the movable end 111 of the wave-guide 11 to move this movable end along the motion plane π. For example, the actuation device 8 can be a micro-motor of stepping type capable of moving the movable end 111 of the wave-guide 11 with movements in the order of the 100 nm.
Preferably, the optoelectronic device 1 comprises a second control loop 902 comprising the photonic circuit 10 and a second control module 94 of the control unit 9 operatively connected to the detector 4 to receive the detection signals SI provided by these latter.
The control module 94 is adapted to receive the detection signals SI and to provide, in response to the aforesaid detection signals, second control signals C2 for the actuation device 8 to move the movable end 111 of the wave-guide 11 and adjust the position of this latter at least along the motion plane π.
The solution illustrated above is very advantageous given that it allows optimization of the transfer of optical power from the light source 2 to the optical coupler 3, in particular when this latter consists of an optical grating coupler (Fig. 5).
By moving the movable end 111 of the wave-guide 11 along a motion plane π, it is possible to align with high precision the light cone exiting from the wave-guide 11 with the active surface 31 of the optical coupler 3. This allows a considerable increase in the measurement resolution of the optoelectronic device.
Moreover, the inventors have verified how the distance Z0 of the motion plane π from the active surface 31 is not critical in order to optimize the transfer of optical power from the light source 2 to the optical coupler 3.
The movement of the movable end 111 can thus take place on a plane rather than three dimensions, with considerable advantages in terms of simple construction and positioning precision.
Preferably, the control unit 9 is adapted to execute a calibration procedure of the position of the movable end 111 of the wave-guide 11 (Fig. 5).
Preferably, the calibration procedure is executed by the second control loop 902.
Preferably, the calibration procedure is executed with the movable end in an initial position P0=X0,Y0 (the coordinate Z0 is preferably maintained fixed for the above reasons).
Preferably, the calibration procedure is executed with the first control loop 901 deactivated and with the light source 2 that initially emits a light radiation LE having a calibration wavelength start at which the optical power SI of the first light radiation L-n received by the first detector 4 takes a maximum absolute value (Fig. 2).
The wavelength start can be obtained acting directly on the light source 2 (for example by means of the control module 93) or on a thermoregulation circuit operatively coupled to the photonic circuit 10.
Preferably, in a first calibration step of the calibration procedure, the control module 94 controls (by means of suitable control signals C2) the actuation device 8 to move the movable end 111 along a first motion axis Y=Y0 of the motion plane π until reaching a first calibration position P1=(X1,Y0) at which the optical power SA of the first light radiation L-π received by the detector 4 takes a maximum value.
Preferably, in a second calibration step of the calibration procedure, the control module 94 controls (by means of suitable control signals C2) the actuation device of 8 to move the movable end 111 along a second motion axis X=X1 of the motion plane π, perpendicular to the aforesaid first motion axis Y0, until reaching a second calibration position P2=(X1,Y1) at which the optical power SA of the first light radiation L-n received by the detector 4 takes a maximum value.
Preferably, in the subsequent steps of the calibration procedure described above, the movement of the movable end 111 is implemented with stepping movements (positive or negative in the order of 100 nm) repeated cyclically until reaching the optimal calibration position along the respective motion axis.
According to a further aspect of the invention, illustrated in the aforesaid figures, the optoelectronic device 1 is provided with a control arrangement to control the temperature of the integrated circuit 100.
Preferably, the optoelectronic device 1 comprises a temperature sensor circuit 71 (preferably integrated with the photonic circuit 10) adapted to provide third detection signals T (of electrical type) indicative of the temperature of the integrated circuit 100.
Preferably, the optoelectronic device 1 comprises a control module 95 (preferably comprised in the control unit 9) and a heating circuit 70 operatively coupled to the integrated circuit 100 to heat this latter, when required.
Preferably, the heating circuit 70 comprises one or more Peltier cells operatively coupled to a voltage source (for example the control unit 9) capable of providing a suitable regulation voltage for the aforesaid cells.
The control module 95, the temperature sensor circuit 71 and heater 70 form a third control loop 903 for regulating the temperature of the integrated circuit 100.
Preferably, the control module 95 is operatively connected to the temperature sensor 71 to receive the detection signals T provided by these latter.
The control module 94 is adapted to receive the detection signals T and to provide, in response to the aforesaid detection signals, third control signals C3 for the heating circuit 70. According to a preferred embodiment, illustrated in the aforesaid figures, the integrated electronic circuit 100 comprises a multilayer structure 100A made of semiconductor material, for example Si (Fig. 4).
The multilayer structure 100A can be produced by means of known techniques for processing semiconductor materials, for example SOI (Silicon On Insulator) wafers.
Preferably, the multilayer structure 100 A comprises a substrate 30 made of semiconductor material (for example Si-bulk having a thickness generally variable from 600um to 200um) Preferably, the multilayer structure 100A comprises a layer of insulating material 20 (for example Si02) superimposed on the substrate 30. For example, the layer of insulating material can be formed by a Buried Oxide Layer of a wafer of SOI type with a thickness comprised between 750 nm and 2 μιη.
Preferably, the multilayer structure 100 A comprises a layer of semiconductor material 10A (for example Si-epi with a thickness between 300 nm and 2 μιη) superimposed on the layer of insulating material 20.
The integrated photonic circuit 10 is advantageously produced at the layer 10A.
The layer 10A of the multilayer structure 100A thus advantageously comprises, in the form of integrated circuits, at least the optical coupler 3, the optical resonator 5, the waveguides 12, 13 and the detectors 4, 6.
Preferably, the temperature sensor circuit 71 is also integrated with the photonic circuit 10 and is produced at the layer 10A of the multilayer structure 100A.
Preferably, the integrated electronic circuit 100 comprises a protective layer 40 made of plastic material superimposed on the layer 10A of the multilayer structure 100A.
The protective layer 40 is advantageously provided with suitable openings to allow the fluid
50 to come into contact with the active surface of the optical resonator 5, to allow optical coupling between the light source 2 and the optical coupler 3 of the photonic circuit 10 and to allow electrical connection between the detectors 4, 6 and the control unit 9.
The optoelectronic device according to the invention has considerable advantages with respect to state of the art devices.
The optoelectronic device 1 uses a closed control loop 901 that allows the light source 2 to emit light radiation with wavelength coupled to the resonance wavelength λτ of the optical resonator 5. As illustrated in Figs. 2-3, the light source 2 is forced to emit light radiation at wavelengths s= -lock for coupling with the resonance wavelength λτ of the optical resonator 2, at which the optical power curves SA, SB take a maximum slope (crossing point P-lock).
This allows a relatively high loop gain to be obtained and therefore considerable improvement of the measurement accuracy and the stability of the feedback control.
The optoelectronic device 1 uses a single optical resonator 5 to generate an error signal of differential type used by the control loop 901 to control the light source 2. This allows a high rejection of any common mode noise (for example due to variations of temperature, vibrations, etc.) to be obtained, with consequent increase of the accuracy and of the measurement resolution.
The optoelectronic device 1 is advantageously provided with a motion system of the waveguide 11 that couples the light source 2 with the photonic circuit 10. It is thus possible to considerably reduce the coupling losses due to any misalignments between the light cone emitted by the wave-guide 11 and the active surface 31 of the optical coupler 3.
The optoelectronic device 1, in particular the photonic circuit 10, and more generally the integrated circuit 100, is particularly suitable for mass production (batch processing) by means of known techniques for processing semiconductor materials. Moreover, the integrated circuit 100, in particular the photonic circuit 10, is easy to operatively couple with the control unit 9. The optoelectronic device 1 therefore has a very compact structure, easy to produce industrially at relatively limited costs.
The optoelectronic device 1 is particularly suitable for use in an apparatus for the detection of substances dispersed in a fluid or in an apparatus of bio-medical type.
An apparatus of this type may comprise, for example, a sample preparation unit to collect a process fluid to analyse, a micro-fluidic chamber and a peristaltic pump to force the collected process fluid to flow from the sample preparation unit into the micro-fluidic chamber.
In the microfluidic chamber, the process fluid is brought into contact with the active surface of the optoelectronic device 1.
The process fluid is conveniently pumped into the microfluidic chamber with suitable speed and flow in order to maximize the binding probability of possible low-concentration target molecules with the active surface 52 of the optoelectronic device 1.
The measurement signals M (which may be indicative of a concentration value or a binding event count) provided by the optoelectronic device 1 may be conveniently processed to obtain an analyte concentration metric by a suitable data-analysis software.
As it adopts a fully differential control system, the optoelectronic device 1 ensures high performance in terms of accuracy and measurement resolution. For example, it is capable of detecting dispersed substances with very low concentration values, for example tens of particles (of dimensions below 100 nm) per millilitre (ml). For many types of target substances, the optoelectronic device 1 is able to offer a numerical count of the molecules in a fluid.

Claims

1. Optoelectronic device (1) for detection of a target substance dispersed in a fluid (50) comprising:
- a light source (2) adapted to emit a light radiation (LE) having a tunable wavelength s;
- an integrated electronic circuit (100) comprising a photonic circuit (10) operatively coupled with said light source;
- a control unit (9) operatively coupled with said light source and said photonic circuit; characterized in that said photonic circuit (10) comprises:
- an optical coupler (3) comprising a first active surface (31) optically coupled with said light source (2) to receive a light radiation (LE) emitted by said light source;
- a first detector (4) optically coupled with said optical coupler (3) to receive a first light radiation (Ln) corresponding to a first portion of a light radiation (LT) transmitted by said optical coupler, said first detector being adapted to provide first detection signals (S I) indicative of an optical power (SA) of said first light radiation (LTi), said first detector being operatively coupled with said control unit (9) to transmit said first detection signals to said control unit;
- an optical resonator (5) optically coupled with said optical coupler (3) to convey and transmit a second light radiation (LT2) corresponding to a second portion of the light radiation (LT) transmitted by said optical coupler, said optical resonator comprising a ring optical path (51) and, in at least a portion of said optical path, a second active surface (52) adapted to come into contact with said fluid (50) and comprising a material capable of selectively absorbing said target substance, a resonance wavelength λΓ of said optical resonator varying as a function of the quantity of said target substance absorbed by said second active surface;
- a second detector (6) optically coupled with said optical resonator (5) to receive the second light radiation (LT2) transmitted by said optical resonator, said second detector being adapted to provide second detection signals (S2) indicative of the optical power (SB) of said second light radiation (LT2), said second detector being operatively coupled with said control unit (9) to transmit said first detection signals to said control unit;
said control unit (9) being adapted to receive and process said first and second detection signals (S 1 , S2) and provide, in response to said first and second detection signals, first control signals (C I) to tune the wavelength s of the light radiation (LE) emitted by said light source (2) so that an optical power difference AS between said first and second light radiation (L-π, LT2) takes a minimum value.
Optoelectronic device, according to claim 1 , wherein said control unit (9) is adapted to provide, in response to said first and second detection signals (S I , S2), first measurement signals (M) indicative of a presence or concentration of said target substance in said fluid (50).
Optoelectronic device, according to any of the previous claims, further comprising a first wave-guide (1 1) adapted to optically couple said optical coupler (3) with said light source (2).
Optoelectronic device, according to any of the previous claims, further comprising a second wave-guide (12) adapted to optically couple said optical coupler (3) with said first detector (4) and said optical resonator (5).
Optoelectronic device, according to any of the previous claims, further comprising a third wave-guide (13) adapted to optically couple said optical resonator (5) with said second detector (6).
Optoelectronic device, according to any of the previous claims, wherein said control unit (9) comprises:
- a measurement module (91) adapted to receive said first and second detection signals (S 1 , S2) and provide, in response to said first and second detection signals, second measurement signals (ASM) indicative of an optical power difference AS between said first and second light radiation (LTi, LT2);
- a signal processing module (92) adapted to receive said second measurement signals (ASM) and provide, in response to said second measurement signals, regulation signals (R) indicative of a reference wavelength for the light radiation (LE) emitted by said light source (2), the optical power difference AS between said first and second light radiation (L-π, LT2) taking a minimum value at said reference wavelength;
- a first control module (93) adapted to receive said regulation signals (R) and provide, in response to said regulation signals, said first control signals (C I).
Optoelectronic device, according to any of the claims from 3 to 6, wherein said first wave-guide (1 1) comprises, in proximal position with respect to the first active surface (3 1) of said optical coupler (3), a movable end (1 1 1) capable of moving at least along a motion plane (π) parallel to said first active surface.
8. Optoelectronic device, according to claim 7, further comprising an actuation device (8) operatively coupled with said movable end (111) to move said movable end along said motion plane (π).
9. Optoelectronic device, according to claim 8, wherein control unit (9) comprises a second control module (94) adapted to receive said first detection signals (SI) and provide, in response to said first detection signals, second control signals (C2) for said actuation device (8) to tune the position of said movable end (111).
10. Optoelectronic device, according to claim 9, wherein said control unit (9) is adapted to execute a calibration procedure of the position of said movable end (111), said calibration procedure comprising:
- a first calibration step, in which said second control module (94) commands said actuation device (8) to move said movable end (111) along a first motion axis (Y0) of said motion plane (π) up to reach a first calibration position (PI) at which the optical power (SA) of the first light radiation (LTi) received from said first detector (4) takes a maximum value;
- a second calibration step, in which said second control module (94) commands said actuation device (8) to move said movable end (111) along a second motion axis (XI) of said motion plane (π), perpendicular to said first motion axis (Y0), up to reach a second calibration position (P2) at which the optical power (SA) of the first light radiation (LTi) received from said first detector (4) takes a maximum value.
11. Optoelectronic device, according to any of the previous claims, wherein said integrated electronic circuit (100) comprises a temperature sensing circuit (71) adapted to provide third detection signals (T) indicative of a temperature of said electronic integrated circuit, said control unit (9) comprising a third control module (95) adapted to receive said third detection signals and provide, in response to said third detection signals, third control signals (C3) for a heating circuit (70) of said optoelectronic device, said heating circuit being operatively coupled with said electronic integrated circuit to heat said electronic integrated circuit.
12. Optoelectronic device, according to any of the previous claims, wherein said light source (2) is a laser light source.
13. Apparatus for detecting a target substance dispersed in a fluid (50) or bio-medical apparatus characterized in that it comprises an optoelectronic device (1), according to any of the previous claims.
14. Bio-medical apparatus characterized in that it comprises an optoelectronic device (1), according to any of the claims from 1 to 12.
PCT/EP2018/051296 2017-01-23 2018-01-19 Optoelectronic device for detection of a substance dispersed in a fluid. WO2018134348A1 (en)

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